# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1332 data_General _audit_creation_date 'Fri Oct 9 14:30:36 1998' _audit_creation_method 'by teXsan' _audit_update_record ? #--------------------------------------------------------------------------- # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #--------------------------------------------------------------------------- # SUBMISSION DETAILS _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? #--------------------------------------------------------------------------- # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #------------------------------------------------------------------------- # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; #--------------------------------------------------------------------------- data_Yamagata_Univ._Dr._Sakiyama #--------------------------------------------------------------------------- # CHEMICAL DATA _chemical_formula_sum 'C50 H64 B Cl3 N2 O9 Zn2 ' _chemical_formula_moiety '?' _chemical_formula_weight 1084.99 _chemical_melting_point ? #--------------------------------------------------------------------------- # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 14.626(1) _cell_length_b 16.343(2) _cell_length_c 13.398(1) _cell_angle_alpha 99.200(2) _cell_angle_beta 114.834(1) _cell_angle_gamma 69.368(4) _cell_volume 2719.7(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10214 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 297.2 #--------------------------------------------------------------------------- _exptl_crystal_description 'platelet' _exptl_crystal_colour 'clear' _exptl_crystal_size_max 0.560 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.160 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.6461 _exptl_absorpt_correction_T_max 1.1329 #--------------------------------------------------------------------------- # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RASA-7 QUANTUM' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 12.195 _diffrn_reflns_number 24447 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9261 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9261 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 #--------------------------------------------------------------------------- # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11564 _reflns_number_gt 6909 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.0859 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6909 _refine_ls_number_parameters 582 _refine_ls_goodness_of_fit_ref 1.439 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00302|Fo|^2^]' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.44 _refine_diff_density_min -0.45 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'B' 'B' 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Zn' 'Zn' 0.284 1.430 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn(1) Zn 0.79242(4) 0.20718(3) 0.80161(4) 0.0592(2) Uani 1.00 d . . . Zn(2) Zn 0.84105(3) 0.38634(3) 0.79653(4) 0.0508(1) Uani 1.00 d . . . Cl(1a) Cl 0.4930(4) 0.1239(3) 1.0113(6) 0.2012 Uiso 0.60 d P . . Cl(1b) Cl 0.5274(7) 0.2399(6) 0.9427(9) 0.2080 Uiso 0.40 d P . . Cl(2a) Cl 0.4284(4) 0.3107(3) 1.0502(5) 0.2012 Uiso 0.60 d P . . Cl(2b) Cl 0.3648(7) 0.2822(5) 1.0289(9) 0.2080 Uiso 0.40 d P . . Cl(3a) Cl 0.2698(3) 0.2245(4) 0.9356(5) 0.2012 Uiso 0.60 d P . . Cl(3b) Cl 0.4674(8) 0.1021(4) 0.984(1) 0.2080 Uiso 0.40 d P . . O(1) O 0.7964(2) 0.2865(2) 0.7058(2) 0.0563(8) Uani 1.00 d . . . O(2) O 0.7518(3) 0.1223(3) 0.8788(3) 0.089(1) Uani 1.00 d . . . O(3) O 0.9021(4) 0.0776(2) 0.7509(4) 0.103(1) Uani 1.00 d . . . O(4) O 0.9034(2) 0.4951(2) 0.8740(3) 0.0639(8) Uani 1.00 d . . . O(5) O 0.6962(2) 0.5023(2) 0.6764(3) 0.079(1) Uani 1.00 d . . . O(6) O 0.6916(3) 0.3055(2) 0.8572(3) 0.078(1) Uani 1.00 d . . . O(7) O 0.7537(2) 0.4174(2) 0.8850(3) 0.0688(9) Uani 1.00 d . . . O(8) O 0.9255(2) 0.2017(2) 0.9329(3) 0.0707(9) Uani 1.00 d . . . O(9) O 0.9781(2) 0.3061(2) 0.9067(3) 0.0642(8) Uani 1.00 d . . . N(1) N 0.6826(3) 0.1578(3) 0.6629(3) 0.075(1) Uani 1.00 d . . . N(2) N 0.8964(2) 0.4056(2) 0.6797(3) 0.0535(9) Uani 1.00 d . . . C(1) C 0.7795(3) 0.2704(2) 0.5987(3) 0.052(1) Uani 1.00 d . . . C(2) C 0.6941(3) 0.2407(3) 0.5289(4) 0.064(1) Uani 1.00 d . . . C(3) C 0.6758(5) 0.2268(4) 0.4188(4) 0.083(2) Uani 1.00 d . . . C(4) C 0.7387(5) 0.2405(4) 0.3749(4) 0.090(2) Uani 1.00 d . . . C(5) C 0.8244(4) 0.2697(3) 0.4457(4) 0.074(1) Uani 1.00 d . . . C(6) C 0.8444(3) 0.2849(3) 0.5562(3) 0.060(1) Uani 1.00 d . . . C(7) C 0.6245(4) 0.2257(3) 0.5764(4) 0.070(1) Uani 1.00 d . . . C(8) C 0.6091(5) 0.1495(5) 0.7058(5) 0.101(2) Uani 1.00 d . . . C(9) C 0.6690(7) 0.0917(6) 0.8064(6) 0.124(3) Uani 1.00 d . . . C(10) C 0.810(1) 0.0855(9) 0.9809(7) 0.203(6) Uani 1.00 d . . . C(11) C 0.7354(6) 0.0716(4) 0.6190(5) 0.097(2) Uani 1.00 d . . . C(12) C 0.8512(7) 0.0547(5) 0.6438(8) 0.139(3) Uani 1.00 d . . . C(13) C 1.0090(8) 0.0614(8) 0.7802(9) 0.191(4) Uani 1.00 d . . . C(14) C 0.7180(9) 0.2232(6) 0.2537(5) 0.143(4) Uani 1.00 d . . . C(15) C 0.9336(3) 0.3188(3) 0.6299(4) 0.058(1) Uani 1.00 d . . . C(16) C 0.9888(3) 0.4357(3) 0.7510(4) 0.063(1) Uani 1.00 d . . . C(17) C 0.9591(4) 0.5147(3) 0.8196(4) 0.070(1) Uani 1.00 d . . . C(18) C 0.8503(4) 0.5713(3) 0.9203(4) 0.078(1) Uani 1.00 d . . . C(19) C 0.8185(3) 0.4695(3) 0.5915(4) 0.065(1) Uani 1.00 d . . . C(20) C 0.7037(3) 0.4858(3) 0.5736(4) 0.070(1) Uani 1.00 d . . . C(21) C 0.5918(4) 0.5262(5) 0.6695(6) 0.110(2) Uani 1.00 d . . . C(22) C 0.6981(3) 0.3791(3) 0.8968(4) 0.066(1) Uani 1.00 d . . . C(23) C 0.6318(5) 0.4253(5) 0.9606(5) 0.100(2) Uani 1.00 d . . . C(24) C 0.9922(3) 0.2411(3) 0.9551(4) 0.061(1) Uani 1.00 d . . . C(25) C 1.0984(5) 0.2061(4) 1.0492(5) 0.094(2) Uani 1.00 d . . . C(26) C 0.2740(3) 0.3051(2) 0.5997(3) 0.0522(9) Uani 1.00 d . . . C(27) C 0.3523(4) 0.3401(3) 0.6077(4) 0.067(1) Uani 1.00 d . . . C(28) C 0.3861(4) 0.3976(4) 0.6903(5) 0.083(2) Uani 1.00 d . . . C(29) C 0.3455(4) 0.4236(4) 0.7695(4) 0.082(1) Uani 1.00 d . . . C(30) C 0.2702(4) 0.3914(3) 0.7647(4) 0.077(1) Uani 1.00 d . . . C(31) C 0.2366(3) 0.3334(3) 0.6825(4) 0.064(1) Uani 1.00 d . . . C(32) C 0.2268(4) 0.1579(3) 0.5612(4) 0.069(1) Uani 1.00 d . . . C(33) C 0.3179(5) 0.1119(3) 0.6472(5) 0.090(2) Uani 1.00 d . . . C(34) C 0.3212(8) 0.0451(4) 0.7031(7) 0.134(3) Uani 1.00 d . . . C(35) C 0.231(1) 0.0229(5) 0.673(1) 0.146(4) Uani 1.00 d . . . C(36) C 0.1370(10) 0.0694(6) 0.5912(9) 0.137(4) Uani 1.00 d . . . C(37) C 0.1356(5) 0.1357(3) 0.5367(6) 0.090(2) Uani 1.00 d . . . C(38) C 0.1070(3) 0.2886(2) 0.4142(3) 0.054(1) Uani 1.00 d . . . C(39) C 0.0431(3) 0.3718(2) 0.4325(3) 0.0515(10) Uani 1.00 d . . . C(40) C -0.0596(3) 0.4112(3) 0.3574(4) 0.060(1) Uani 1.00 d . . . C(41) C -0.1019(3) 0.3692(4) 0.2599(4) 0.075(1) Uani 1.00 d . . . C(42) C -0.0407(4) 0.2885(4) 0.2400(4) 0.088(2) Uani 1.00 d . . . C(43) C 0.0582(4) 0.2500(3) 0.3142(4) 0.079(1) Uani 1.00 d . . . C(44) C 0.3022(3) 0.2003(2) 0.4291(3) 0.0505(9) Uani 1.00 d . . . C(45) C 0.3711(3) 0.1151(2) 0.4320(3) 0.054(1) Uani 1.00 d . . . C(46) C 0.4312(3) 0.0874(3) 0.3686(4) 0.063(1) Uani 1.00 d . . . C(47) C 0.4258(3) 0.1435(3) 0.2990(4) 0.065(1) Uani 1.00 d . . . C(48) C 0.3597(4) 0.2284(3) 0.2933(4) 0.071(1) Uani 1.00 d . . . C(49) C 0.3003(3) 0.2554(3) 0.3579(4) 0.065(1) Uani 1.00 d . . . C(50a) C 0.3973(4) 0.2253(3) 0.9567(4) 0.2012 Uiso 0.60 d P . . C(50b) C 0.4205(5) 0.2111(5) 0.9401(6) 0.2080 Uiso 0.40 d P . . B(1) B 0.2284(3) 0.2373(3) 0.5020(4) 0.052(1) Uani 1.00 d . . . H(3) H 0.6176 0.2071 0.3717 0.1001 Uiso 1.00 calc . . . H(5) H 0.8692 0.2792 0.4171 0.0891 Uiso 1.00 calc . . . H(7a) H 0.5695 0.2079 0.5185 0.0841 Uiso 1.00 calc . . . H(7b) H 0.5943 0.2792 0.6077 0.0841 Uiso 1.00 calc . . . H(8a) H 0.5720 0.2059 0.7255 0.1211 Uiso 1.00 calc . . . H(8b) H 0.5597 0.1244 0.6504 0.1211 Uiso 1.00 calc . . . H(9a) H 0.6968 0.0329 0.7855 0.1482 Uiso 1.00 calc . . . H(9b) H 0.6227 0.0947 0.8407 0.1482 Uiso 1.00 calc . . . H(10a) H 0.8657 0.1100 1.0207 0.2435 Uiso 1.00 calc . . . H(10b) H 0.7653 0.0969 1.0197 0.2435 Uiso 1.00 calc . . . H(10c) H 0.8396 0.0241 0.9731 0.2435 Uiso 1.00 calc . . . H(11a) H 0.7303 0.0260 0.6504 0.1160 Uiso 1.00 calc . . . H(11b) H 0.6982 0.0706 0.5414 0.1160 Uiso 1.00 calc . . . H(12a) H 0.8566 0.0883 0.5961 0.1669 Uiso 1.00 calc . . . H(12b) H 0.8835 -0.0057 0.6326 0.1669 Uiso 1.00 calc . . . H(13a) H 1.0402 0.0786 0.8547 0.2291 Uiso 1.00 calc . . . H(13b) H 1.0421 0.0007 0.7717 0.2291 Uiso 1.00 calc . . . H(13c) H 1.0186 0.0937 0.7344 0.2291 Uiso 1.00 calc . . . H(14a) H 0.7790 0.1808 0.2464 0.1711 Uiso 1.00 calc . . . H(14b) H 0.6590 0.2021 0.2188 0.1711 Uiso 1.00 calc . . . H(14c) H 0.7030 0.2760 0.2201 0.1711 Uiso 1.00 calc . . . H(15a) H 0.9700 0.3239 0.5881 0.0697 Uiso 1.00 calc . . . H(15b) H 0.9809 0.2783 0.6873 0.0697 Uiso 1.00 calc . . . H(16a) H 1.0418 0.3896 0.7987 0.0754 Uiso 1.00 calc . . . H(16b) H 1.0164 0.4499 0.7057 0.0754 Uiso 1.00 calc . . . H(17a) H 0.9145 0.5641 0.7739 0.0836 Uiso 1.00 calc . . . H(17b) H 1.0212 0.5265 0.8723 0.0836 Uiso 1.00 calc . . . H(18a) H 0.8152 0.5558 0.9566 0.0931 Uiso 1.00 calc . . . H(18b) H 0.9006 0.5975 0.9718 0.0931 Uiso 1.00 calc . . . H(18c) H 0.7995 0.6115 0.8636 0.0931 Uiso 1.00 calc . . . H(19a) H 0.8331 0.5235 0.6109 0.0785 Uiso 1.00 calc . . . H(19b) H 0.8269 0.4478 0.5247 0.0785 Uiso 1.00 calc . . . H(20a) H 0.6832 0.4358 0.5401 0.0842 Uiso 1.00 calc . . . H(20b) H 0.6585 0.5349 0.5276 0.0842 Uiso 1.00 calc . . . H(21a) H 0.5919 0.5368 0.7414 0.1323 Uiso 1.00 calc . . . H(21b) H 0.5497 0.5777 0.6274 0.1323 Uiso 1.00 calc . . . H(21c) H 0.5630 0.4802 0.6352 0.1323 Uiso 1.00 calc . . . H(23a) H 0.6523 0.3914 1.0223 0.1196 Uiso 1.00 calc . . . H(23b) H 0.6417 0.4806 0.9851 0.1196 Uiso 1.00 calc . . . H(23c) H 0.5590 0.4335 0.9151 0.1196 Uiso 1.00 calc . . . H(25a) H 1.1415 0.2411 1.0589 0.1128 Uiso 1.00 calc . . . H(25b) H 1.0877 0.2077 1.1147 0.1128 Uiso 1.00 calc . . . H(25c) H 1.1328 0.1475 1.0330 0.1128 Uiso 1.00 calc . . . H(27) H 0.3826 0.3235 0.5543 0.0800 Uiso 1.00 calc . . . H(28) H 0.4389 0.4197 0.6924 0.0990 Uiso 1.00 calc . . . H(29) H 0.3695 0.4632 0.8265 0.0984 Uiso 1.00 calc . . . H(30) H 0.2402 0.4090 0.8184 0.0926 Uiso 1.00 calc . . . H(31) H 0.1846 0.3114 0.6826 0.0769 Uiso 1.00 calc . . . H(33) H 0.3809 0.1267 0.6687 0.1086 Uiso 1.00 calc . . . H(34) H 0.3850 0.0156 0.7612 0.1603 Uiso 1.00 calc . . . H(35) H 0.2330 -0.0243 0.7078 0.1746 Uiso 1.00 calc . . . H(36) H 0.0737 0.0558 0.5727 0.1640 Uiso 1.00 calc . . . H(37) H 0.0706 0.1668 0.4810 0.1075 Uiso 1.00 calc . . . H(39) H 0.0711 0.4024 0.4987 0.0618 Uiso 1.00 calc . . . H(40) H -0.1005 0.4673 0.3736 0.0717 Uiso 1.00 calc . . . H(41) H -0.1717 0.3956 0.2078 0.0896 Uiso 1.00 calc . . . H(42) H -0.0682 0.2589 0.1727 0.1061 Uiso 1.00 calc . . . H(43) H 0.0968 0.1932 0.2972 0.0945 Uiso 1.00 calc . . . H(45) H 0.3771 0.0744 0.4795 0.0646 Uiso 1.00 calc . . . H(46) H 0.4767 0.0286 0.3735 0.0753 Uiso 1.00 calc . . . H(47) H 0.4669 0.1241 0.2555 0.0782 Uiso 1.00 calc . . . H(48) H 0.3546 0.2685 0.2456 0.0852 Uiso 1.00 calc . . . H(49) H 0.2559 0.3145 0.3534 0.0777 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn(1) 0.0797(3) 0.0624(3) 0.0564(3) -0.0451(2) 0.0296(2) -0.0097(2) Zn(2) 0.0577(3) 0.0487(3) 0.0538(3) -0.0297(2) 0.0192(2) -0.0066(2) O(1) 0.079(2) 0.063(2) 0.048(1) -0.048(1) 0.026(1) -0.012(1) O(2) 0.126(3) 0.100(3) 0.074(2) -0.072(2) 0.037(2) 0.004(2) O(3) 0.118(3) 0.077(2) 0.092(3) -0.021(2) 0.035(2) -0.025(2) O(4) 0.067(1) 0.050(1) 0.075(2) -0.032(1) 0.017(1) -0.008(1) O(5) 0.056(2) 0.097(2) 0.079(2) -0.021(2) 0.016(1) 0.012(2) O(6) 0.089(2) 0.085(2) 0.096(3) -0.048(2) 0.058(2) -0.024(2) O(7) 0.080(2) 0.071(2) 0.074(2) -0.038(1) 0.040(2) -0.021(1) O(8) 0.089(2) 0.074(2) 0.061(2) -0.047(2) 0.019(1) 0.003(1) O(9) 0.067(2) 0.059(2) 0.069(2) -0.034(1) 0.014(1) 0.005(1) N(1) 0.104(3) 0.087(3) 0.066(2) -0.075(2) 0.030(2) -0.017(2) N(2) 0.058(2) 0.049(2) 0.063(2) -0.027(1) 0.020(1) 0.003(1) C(1) 0.067(2) 0.051(2) 0.050(2) -0.033(2) 0.024(2) -0.008(2) C(2) 0.079(2) 0.070(3) 0.056(2) -0.046(2) 0.021(2) -0.006(2) C(3) 0.112(4) 0.094(3) 0.054(3) -0.068(3) 0.013(2) -0.006(2) C(4) 0.144(5) 0.102(4) 0.052(3) -0.077(4) 0.037(3) -0.011(3) C(5) 0.102(3) 0.079(3) 0.066(3) -0.046(3) 0.042(2) -0.007(2) C(6) 0.082(2) 0.057(2) 0.056(2) -0.036(2) 0.031(2) -0.007(2) C(7) 0.080(3) 0.088(3) 0.063(3) -0.058(2) 0.023(2) -0.011(2) C(8) 0.120(4) 0.147(5) 0.085(4) -0.104(4) 0.033(3) -0.001(4) C(9) 0.171(6) 0.161(7) 0.096(5) -0.135(6) 0.037(4) 0.000(4) C(10) 0.29(1) 0.29(1) 0.085(5) -0.22(1) 0.001(7) 0.055(7) C(11) 0.150(5) 0.079(3) 0.084(4) -0.078(4) 0.038(4) -0.022(3) C(12) 0.148(6) 0.091(4) 0.148(7) -0.034(4) 0.044(5) -0.047(5) C(13) 0.121(6) 0.20(1) 0.159(9) 0.021(6) 0.040(6) -0.054(8) C(14) 0.247(10) 0.182(8) 0.061(4) -0.143(8) 0.068(5) -0.030(4) C(15) 0.065(2) 0.058(2) 0.067(2) -0.026(2) 0.033(2) -0.002(2) C(16) 0.062(2) 0.066(2) 0.076(3) -0.038(2) 0.024(2) 0.002(2) C(17) 0.073(2) 0.061(2) 0.081(3) -0.041(2) 0.017(2) 0.001(2) C(18) 0.074(2) 0.054(2) 0.086(3) -0.024(2) 0.013(2) -0.018(2) C(19) 0.075(2) 0.055(2) 0.071(3) -0.029(2) 0.020(2) 0.013(2) C(20) 0.069(2) 0.075(3) 0.064(3) -0.031(2) 0.009(2) 0.019(2) C(21) 0.061(3) 0.146(6) 0.112(5) -0.012(3) 0.029(3) 0.021(4) C(22) 0.070(2) 0.085(3) 0.054(2) -0.036(2) 0.029(2) -0.017(2) C(23) 0.101(4) 0.137(5) 0.089(4) -0.060(4) 0.058(3) -0.047(4) C(24) 0.067(2) 0.055(2) 0.058(2) -0.024(2) 0.018(2) -0.001(2) C(25) 0.091(3) 0.100(4) 0.083(4) -0.035(3) 0.011(3) 0.026(3) C(26) 0.047(2) 0.048(2) 0.051(2) -0.002(1) 0.016(1) 0.005(2) C(27) 0.078(3) 0.065(2) 0.065(3) -0.026(2) 0.033(2) -0.006(2) C(28) 0.085(3) 0.092(3) 0.086(4) -0.043(3) 0.037(3) -0.011(3) C(29) 0.066(3) 0.088(3) 0.073(3) -0.023(2) 0.016(2) -0.022(3) C(30) 0.063(2) 0.094(3) 0.056(3) -0.008(2) 0.023(2) -0.017(2) C(31) 0.061(2) 0.069(2) 0.058(2) -0.012(2) 0.024(2) 0.000(2) C(32) 0.092(3) 0.047(2) 0.084(3) -0.011(2) 0.056(3) -0.004(2) C(33) 0.112(4) 0.066(3) 0.099(4) 0.012(3) 0.066(3) 0.029(3) C(34) 0.201(8) 0.078(4) 0.139(6) 0.023(5) 0.120(7) 0.044(4) C(35) 0.24(1) 0.070(4) 0.20(1) -0.027(6) 0.165(10) 0.011(5) C(36) 0.224(10) 0.103(5) 0.171(8) -0.084(6) 0.135(8) -0.019(6) C(37) 0.126(4) 0.068(3) 0.114(4) -0.043(3) 0.076(4) -0.016(3) C(38) 0.056(2) 0.052(2) 0.061(2) -0.018(2) 0.027(2) -0.002(2) C(39) 0.054(2) 0.047(2) 0.058(2) -0.018(2) 0.021(2) 0.005(2) C(40) 0.052(2) 0.062(2) 0.070(3) -0.016(2) 0.023(2) 0.013(2) C(41) 0.054(2) 0.093(3) 0.071(3) -0.025(2) 0.011(2) 0.011(2) C(42) 0.083(3) 0.117(4) 0.064(3) -0.047(3) 0.021(2) -0.023(3) C(43) 0.070(2) 0.076(3) 0.077(3) -0.024(2) 0.023(2) -0.025(2) C(44) 0.051(2) 0.044(2) 0.053(2) -0.010(1) 0.019(2) -0.002(2) C(45) 0.060(2) 0.042(2) 0.061(2) -0.017(2) 0.024(2) -0.007(2) C(46) 0.061(2) 0.052(2) 0.079(3) -0.016(2) 0.035(2) -0.016(2) C(47) 0.062(2) 0.077(3) 0.060(3) -0.020(2) 0.030(2) -0.008(2) C(48) 0.079(3) 0.072(3) 0.067(3) -0.010(2) 0.037(2) 0.017(2) C(49) 0.075(2) 0.056(2) 0.062(3) -0.003(2) 0.035(2) 0.011(2) B(1) 0.053(2) 0.044(2) 0.057(2) -0.009(2) 0.025(2) -0.002(2) #--------------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #--------------------------------------------------------------------------- _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn(1) Zn(2) 3.2644(7) . . yes Zn(1) O(1) 1.995(4) . . yes Zn(1) O(2) 2.214(5) . . yes Zn(1) O(3) 2.362(4) . . yes Zn(1) O(6) 2.045(4) . . yes Zn(1) O(8) 1.985(3) . . yes Zn(1) N(1) 2.148(4) . . yes Zn(2) O(1) 2.003(3) . . yes Zn(2) O(4) 2.197(3) . . yes Zn(2) O(5) 2.440(3) . . yes Zn(2) O(7) 1.979(4) . . yes Zn(2) O(9) 2.048(2) . . yes Zn(2) N(2) 2.146(4) . . yes O(1) C(1) 1.348(5) . . yes O(2) C(9) 1.394(10) . . yes O(2) C(10) 1.37(1) . . yes O(3) C(12) 1.371(10) . . yes O(3) C(13) 1.38(1) . . yes O(4) C(17) 1.433(8) . . yes O(4) C(18) 1.420(6) . . yes O(5) C(20) 1.403(7) . . yes O(5) C(21) 1.402(7) . . yes O(6) C(22) 1.253(6) . . yes O(7) C(22) 1.256(8) . . yes O(8) C(24) 1.262(7) . . yes O(9) C(24) 1.243(6) . . yes N(1) C(7) 1.489(7) . . yes N(1) C(8) 1.47(1) . . yes N(1) C(11) 1.509(7) . . yes N(2) C(15) 1.488(5) . . yes N(2) C(16) 1.488(5) . . yes N(2) C(19) 1.486(5) . . yes C(1) C(2) 1.404(6) . . yes C(1) C(6) 1.391(8) . . yes C(2) C(3) 1.380(7) . . yes C(2) C(7) 1.506(9) . . yes C(3) C(4) 1.37(1) . . yes C(4) C(5) 1.406(9) . . yes C(4) C(14) 1.519(9) . . yes C(5) C(6) 1.382(7) . . yes C(6) C(15) 1.495(6) . . yes C(8) C(9) 1.52(1) . . yes C(11) C(12) 1.51(1) . . yes C(16) C(17) 1.504(7) . . yes C(19) C(20) 1.522(7) . . yes C(22) C(23) 1.488(9) . . yes C(24) C(25) 1.514(6) . . yes C(26) C(27) 1.411(8) . . yes C(26) C(31) 1.382(7) . . yes C(26) B(1) 1.646(6) . . yes C(27) C(28) 1.373(7) . . yes C(28) C(29) 1.367(9) . . yes C(29) C(30) 1.354(9) . . yes C(30) C(31) 1.376(7) . . yes C(32) C(33) 1.397(6) . . yes C(32) C(37) 1.40(1) . . yes C(32) B(1) 1.636(8) . . yes C(33) C(34) 1.40(1) . . yes C(34) C(35) 1.37(2) . . yes C(35) C(36) 1.39(1) . . yes C(36) C(37) 1.39(2) . . yes C(38) C(39) 1.403(5) . . yes C(38) C(43) 1.396(6) . . yes C(38) B(1) 1.659(5) . . yes C(39) C(40) 1.392(4) . . yes C(40) C(41) 1.377(6) . . yes C(41) C(42) 1.367(8) . . yes C(42) C(43) 1.351(6) . . yes C(44) C(45) 1.396(4) . . yes C(44) C(49) 1.399(7) . . yes C(44) B(1) 1.649(7) . . yes